CN1054268A - The method of extraction and recovery gold - Google Patents

The method of extraction and recovery gold Download PDF

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Publication number
CN1054268A
CN1054268A CN91101164A CN91101164A CN1054268A CN 1054268 A CN1054268 A CN 1054268A CN 91101164 A CN91101164 A CN 91101164A CN 91101164 A CN91101164 A CN 91101164A CN 1054268 A CN1054268 A CN 1054268A
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gold
thiocarbamide
acid
synergist
leaching
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CN91101164A
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CN1030720C (en
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克雷格·克林顿·肯纳
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Rio Tinto Services Ltd
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CRA Services Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/16—Extraction of metal compounds from ores or concentrates by wet processes by leaching in organic solutions
    • C22B3/1608—Leaching with acyclic or carbocyclic agents
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/16—Extraction of metal compounds from ores or concentrates by wet processes by leaching in organic solutions
    • C22B3/1666—Leaching with heterocyclic compounds
    • C22B3/1675—Leaching with a mixture of organic agents wherein one agent at least is a heterocyclic compounds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Abstract

Hydrometallurgy reclaims the method for gold from gold-bearing material, wherein comprises the step with the acid lixiviant solution-treated gold-bearing material that contains thiocarbamide and iron ion, it is characterized in that also containing in this solution a kind of Synergist S-421 95 of iron ion, thereby obviously reduces the loss of thiocarbamide.This Synergist S-421 95 can be selected from: dicarboxylic acid and tricarboxylic acid, phosphoric acid and phosphoric acid salt, thiocyanate-, fluorochemical, silicofluoric acid and silicofluoride, EDTA and edta salt, and their mixture.

Description

The method of extraction and recovery gold
The present invention relates to from gold-bearing material, extract and reclaim the method for gold.This class material comprises gold containing ore, concentrate, the anode sludge and residue, contains golden scrap metal, and the material that leaches or separate out other technical finesse of gold previously with roasting, bacterium leaching, pressure from gangue.
The present invention relates to from gold-bearing material (as above-mentioned material) with following lixiviation process extraction and reclaim gold: continuously or intermittently stirring tank stirs, and vat leaches, and resembles that pit leaches and the lixiviation process on the spot of heap leaching and so on or solution mining lixiviation process on the spot.
At present, almost generally adopt conventional prussiate lixiviation process extraction gold.But, the safety that increases day by day that the use prussiate brings and the pressure of environmental hazard; Add that the prussiate lixiviation process is being restricted aspect those unmanageable Gold Ores of processing (as high-melting-point sulfide ore, carbonaceous ore, contain the ore of a certain amount of prussiate).Therefore, be necessary other feasible on exploiting economy lixiviation process.
Knownly make oxygenant with Manganse Dioxide, hydrogen peroxide or iron ion, gold can be dissolved in (D.W.Bilston in the acidifying thiourea solution apace, R.N.Millet and J.T.Woodcock(1987) " research and development of lyometallurgy " procceedings (Australia mining emtallurgy research institute, Melbourne) 19-28 page or leaf).But this gold dissolution method is seldom used in gold industry.The major obstacle of using this method is: the oxidative degradation of thiocarbamide generation over-drastic is being arranged under the situation of above-mentioned oxygenant.Relevant chemical reaction can change into curing carbonamidine and (2) and then irreversibly be decomposed into these two reaction formula of sulphur, cyanamide and thiocarbamide and show with (1) initial oxygen
Tu=thiocarbamide in the formula, (tu) 2+ 2=curing carbonamidine.
(1) speed of reaction is faster than (2), is a principal reaction of the relative consumption of decision thiocarbamide.And the passivation of gold often takes place simultaneously with the quick consumption of thiocarbamide in the lixiviation process charging, thereby causes the reduction of the gold rate of recovery.Therefore, compare with the cyanide process of generally acknowledging, it is very not noticeable that thiourea leaching process seems.
Recent research work shows, thiocarbamide and sulfurous gas and usefulness, the loss of its oxidative degradation can obviously reduce (R.G.Schulze(1984) U.S. metal magazine 36 volumes 6 phase 62-65 pages or leaves).But in fact with sulfurous gas reduce the consumption of thiocarbamide might not be always (the D.W.Bilston of success, R.N.Millet and J.T.Woodcock(1987) " research and development of lyometallurgy " procceedings (Australia mining emtallurgy research institute, Melbourne) 19-28 page or leaf).Above-mentioned researchist has also proposed to use instead a kind of substituting thioureido, the i.e. patent application of ethylene thiourea.Ethylene thiourea has bigger oxidative stability and great anti-oxidant degradation property (R.G.Schulze(1983) German Patent 3347165 than thiocarbamide).But as surrogate, the cost of ethylene thiourea is also too high.
The present invention is with the following basis that is found to be.Promptly by a kind of in acidic solution to Fe 3+The chemical reagent that mating capability is arranged can reduce the oxidative degradation of thiocarbamide significantly.
Therefore, the invention provides a kind of from gold-bearing material hydrometallurgy reclaim the method for gold.This method comprises the step of handling gold-bearing material with the acid lixiviant solution that contains thiocarbamide and iron ion, it is characterized in that containing in this solution a kind of Synergist S-421 95 of iron ion.
Make Fe 3+Ionic oxidation capacity or oxidizing intensity are reduced to such degree, and promptly gold still dissolves with sizable speed, and thiocarbamide is because of Fe 3+Oxidative degradation but obviously reduce.
Fe is being arranged 3+Under the situation of above-mentioned chemical reagent, in the solution with Au(Tu) 1+The gold that ionic species exists can reclaim by enough following known technologies: adsorb on gac or resin, tie with iron or with aluminium glue, with electrolytic metallurgy, hydrogen reducing or the solvent extraction of porous carbon electrodes.Therefore, the present invention extends to extraction and the method that reclaims gold from gold-bearing material always.
The present invention is different from the prior art in this area, because key of the present invention is autotelic Fe 3+Coordination reaction, purpose are to reduce Fe 3+Oxidizing power, the result is that the oxidational losses of thiocarbamide obviously reduces.The main contents of other patent of this area are as follows:
English Patent GB 2 152 488 R.Schulze(SKW Trostberg)
Relate to the Synergist S-421 95 of cyclic thiourea derivative as gold.Relevant cyclic thiourea is ethylene thiourea and propylidene thiocarbamide.Compare with thiocarbamide, cyclic thiourea has bigger anti-oxidant degradation property, and still has good gold ligand reactivity and gold leaching rate.
U.S. Pat 4 561 947 R.Schulze(SKW Trostberg)
Relate to sulfurous gas and (or provide SO 2Other compound in source is such as sulphite, hydrosulphite, pyrosulfite etc.) as regeneration " aminoiminomethanesulfonic acid " (as curing carbonamidine) reductive agent.In leaching process, SO 2, thiocarbamide and a kind of oxygenant (be generally Fe 3+) and usefulness, be controlled at a preset value leaching electromotive force, this moment precious metal higher and degraded thiocarbamide of the leaching rate degree that minimizes.In this invention, leaching electromotive force is by SO 2Come stepless control.People expect SO 2At first play most of Fe wherein 3+Be reduced into Fe 3+Effect.The value that leaches electromotive force is determining Fe 3+Be reduced into Fe 2+Limit.Because the chemical reaction of this invention, the main oxygenant that exists under typical leaching condition is the curing carbonamidine.This invention does not relate to Fe 3+Coordination reaction.
English Patent GB 2 181 722 R.H.Little
Relate to thiocarbamide and urea and lignin sulfonic acid potassium and be used for extraction and recovery precious metal.Above-claimed cpd is not clear in the effect that thiocarbamide leaches in the reaction.But, by these compounds " co-adsorption " on gac and carry the high-carbon cation exchange property, thereby improve the efficient that reclaims precious metal/thiourea complex with gac, realize the recovery of precious metal in the thiourea solution.Urea and lignin sulfonic acid potassium can not form tangible title complex with iron ion, so this English Patent and the present invention do not have similarity.
People (Anglo American Corp.ofSth.Afr.) such as south african patent ZA 85/4463B.K.Loveday
Relate to the solution that enables to dissolve gold and pass diapire, from diapire fines, diapire slit and crackle, leach and reclaim the method for gold on the spot.By using a kind of 0.2-1.0g/l of containing thiocarbamide and optional 0.75g/lFe 3+And 1.3g/lNa 2So 3Acidic solution leach gold.Be collected in the storage tank so that the recirculation use using solution.The solution that will contain gold reclaims dissolved gold by activated carbon column.This south african patent only relates to leaching-out technique, does not propose what clear and definite new leaching reaction.
In brief, for leaching gold having under the situation of thiocarbamide, have greater than 380mv(standard hydrogen electrode N.H.E.) the leaching electromotive force.But, if leach electromotive force greater than 420mv(to N.H.E.), can cause the oxidation of thiocarbamide again.The Fe of Pei Heing not 3+The ionic oxidation potential is that 770mv(is to N.H.E.), so as expected, the Fe that does not cooperate is being arranged 3+Under the situation, gold and thiocarbamide are all oxidized.By Fe 3+Coordination reaction, make Fe 3+Oxidation potential be significantly less than 770mv(to N.H.E.), gold is still with sizable speed oxidation, and the oxidation loss of thiocarbamide obviously reduces.In actually operating, oxidation potential be preferably in 390 and 500mv(to N.H.E.) between.
In acidic solution, i.e. pH＜7 o'clock, Fe 3+Coordination reaction can realize by chemical compound lot.Commercially available salt can be used as Fe 3+Synergist S-421 95, some raw product (are generally Fe 3+The mixture of Synergist S-421 95) also can be used to be made into Fe 3+Synergist S-421 95.For example, make raw product, even the cellulosic materials oxidation generates polyvalent alcohol, the complex mixture of hydroxycarboxylic acid and carboxylic acid with chemical process.This mixture can be used as coordination solution, satisfies needs of the present invention.Perhaps make raw product with biological method, promptly with the microorganism that resembles aspergillus niger (Aspergillus niger) class make can with Fe 3+The carboxylic acid of coordination reaction takes place, as citric acid.
Some Fe 3+Synergist S-421 95 list in table 1.
The Synergist S-421 95 of preferentially selecting for use can form stability constant logK＞1, some compounds of iron complex preferably＞2.0.
" Chemistry Of the Metal Chelate Compounds " (the U.S. copyright 1952) that Martell and Calvin write and " Sta bility Constants of metal-Ion Complexes " supplement NO.1, special interest publishing NO.25(American Chemical Society publishes, u.S. copyright 1971) provide the practicality compilation data of stability constant of the Synergist S-421 95 of multiple iron.
Table 2 general introduction modified version Fe 3+/ thiocarbamide gold leaches system and (promptly uses coordination Fe 3+) general leaching condition.The condition and range of enumerating in the table 2 is applicable to whole Fe listed in the table 1 3+Synergist S-421 95.
There is being or do not having Fe 3+Under the situation of Synergist S-421 95 (being oxalic acid), Fe 3+See Fig. 1 with the comparison diagram of thiocarbamide speed of reaction.That point of relative thiocarbamide consumption 100% among the figure is regarded as Fe 3+Ion Restore All becomes Fe 2+Ion.
Clearly, by making Fe with oxalic acid generation coordination reaction 3+The practice that weakens of oxidizing intensity telling on aspect the thiocarbamide consumption reducing.Fe 3+Although reduced the consumption of thiocarbamide with the coordination reaction of oxalic acid, yet what adverse influence gold leaching reaction do not had.The Fig. 2 that detects gold rotating disc electrode dissolving situation has illustrated this point.Do not having under the situation of oxalic acid, the dissolution rate of gold constantly reduces along with the prolongation of solution time limit of service.
After 20 hours, the dissolution rate of gold significantly reduces (promptly reducing about 73%), and dun appears in the gold surface simultaneously, and this shows the passivation that certain form occurs.In contrast, having under the situation of oxalic acid, along with the prolongation of solution time limit of service, it is very slow that the dissolution rate of gold reduces.For example, 960 hours (promptly 40 days) afterwards, the dissolution rate of gold only reduces 40%.The gold surface still keeps light, does not have the sign of passivation.
Modified version Fe 3+/ thiocarbamide gold leaches system and also can use in the pillar leaching experiment, and purpose is to simulate the heap leaching of gold containing ore.Its leaching condition is summarized as follows:
General pillar leaching condition
Ore type High-melting-point, low-grade yellow iron (about 7kg classification 1.2PPm gold)
The ore pre-treatment In the ore packed column, carry out biological heap leaching simulation.Before carrying out the gold leaching, the target of setting is about＞80% oxidation of pyrite.
Gold leaches (room temperature) Soak ore to stablize Fe with the sulphuric acid soln that contains oxalate earlier 3+Concentration.At Fe 3+Concentration stabilize after, in leaching agent solution, add thiocarbamide.
The gold leaching agent Fe 3+About 0.005M oxalic acid 0.056M H 2SO 40.100M thiocarbamide 0.065M
Infiltration rate About 32ml/hr(is on average above 32 days)
The pillar leaching experiment is the result be summarized in the table 3.Gold extraction (%) is seen Fig. 3 to the relation curve of fate.From the 27th day (when promptly stopping to add thiocarbamide) extrapolation, show about 43 days after (if thiocarbamide in whole process continuously add), the expection rate of recovery is about 80%.
In a word, concerning gold recovery, leaching rate and thiocarbamide consumed, experimental result all was very favorable.This technology also has potential value to handling low-grade gold containing ore (had acidity originally or will carry out acidity pretreated, as bio-oxidation etc.).Because will carry out costliness and the neutralization reaction processing of poor efficiency often, owing to make a large amount of losses of prussiate unavoidably, so in these cases, the application of conventional alkaline cyanide process is restricted.
Also can realize leaching system recoveries gold by the method that gold is glued on the iron powder with modified version acid/thiocarbamide.Other method (G.Deschnes(1986) The Canadian Mining ﹠amp; Metal-lurgical Bulletin 79 volume 76-83 pages or leaves) such as be adsorbed on the charcoal, electrolytic metallurgy, solvent extraction, hydrogen reducing or be suitable for too with the lead powder gluing.In a model experiment, iron powder added to contain 100ppm Au(tu) 2+, in 0.066M thiocarbamide, 0.1M sulfuric acid and the 0.05M oxalic acid solution.There is the gold of 90% dissolved state to be separated out after 30 minutes approximately by gluing.
Table 1: be applicable to modified version Fe 3+/ thiocarbamide gold leaches the acidproof Fe of system 3+Synergist S-421 95
General type instance
Dicarboxylic acid and tricarboxylic oxalic acid and oxalate, citric acid and Citrate trianion, tartrate and tartrate
Hydrochlorate, glyconic acid and gluconate.
Phosphoric acid class phosphorylating reagent and phosphoric acid salt, orthophosphoric acid salt, pyrophosphate salt, polyphosphate.
Thiocyanate-ammonium thiocyanate, Sodium Thiocyanate 99.
Fluorochemical hydrofluoric acid, Sodium Fluoride.
Silicofluoride silicofluoric acid, silicofluoride.
EDTA ethylenediamine tetraacetic acid (EDTA), edta salt.
Table 2: modified version Fe 3+/ thiocarbamide gold leaches the general condition of system
The variable condition
Fe 3+0.0025-0.1M
Thiocarbamide 0.005-0.4M, preferably 0.02-0.4M
PH?????????????0.5-4.5
Electromotive force 350-700mV(is to standard hydrogen electrode)
Fe 3+Cooperate 0.01-1.0M, preferably 0.01-0.2M
Agent
Temperature 10-90C
Table 3: use modified version Fe 3+/ thiocarbamide leaches the pillar leaching test result of system
Fate gold extraction (%)
5??18.0
10??36.1
15??45.7
22??57.9
32??68.7
Attention: stop to add thiocarbamide after 1.27 days
2.32 it back thiocarbamide reclaims %=98%
Obviously, scope of the present invention is not subjected to the restriction of the detail that above relates to.

Claims (6)

1, a kind of from gold-bearing material hydrometallurgy reclaim the method for gold, wherein comprise step with the acid lixiviant solution-treated gold-bearing material that contains thiocarbamide and iron ion, it is characterized in that also containing in this solution the Synergist S-421 95 of iron ion.
2, be selected from dicarboxylic acid and tricarboxylic acid, phosphoric acid and phosphoric acid salt, thiocyanate-, fluorochemical, silicofluoric acid and silicofluoride, EDTA and edta salt and their mixture according to the Synergist S-421 95 that the process of claim 1 wherein.
3, according to the method for claim 1 or claim 2, wherein treatment temp is in 10-90 ℃ of scope, and the PH of leaching agent solution contains 0.0025-0.1MFe in the 0.5-4.5 scope 3+, 0.005-0.4M thiocarbamide and 0.01-1.0MFe 3+Synergist S-421 95, the leaching electromotive force of leaching agent solution at 350-700mV(to standard hydrogen electrode) in the scope.
4, according to the method for claim 3, wherein leach electromotive force at 390-500mV(to standard hydrogen electrode) in the scope.
5, according to the method for above-mentioned any one claim, wherein Synergist S-421 95 generates stability constant logK greater than 1 iron complex.
6, according to the method for claim 5, Synergist S-421 95 wherein comprises oxalic acid.
CN91101164A 1990-02-23 1991-02-23 Extraction and recovery of gold Expired - Fee Related CN1030720C (en)

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CN103276206B (en) * 2013-06-09 2014-07-02 中南大学 Method for leaching gold in alkaline thiourea system efficiently and stably
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CN111517534A (en) * 2020-04-15 2020-08-11 安徽大地熊新材料股份有限公司 Waste acid recycling process
CN111517534B (en) * 2020-04-15 2022-07-05 安徽大地熊新材料股份有限公司 Waste acid recycling process

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US5260040A (en) 1993-11-09
BR9104641A (en) 1992-03-24
GB9119973D0 (en) 1991-11-27
WO1991013177A1 (en) 1991-09-05
GB2248632A (en) 1992-04-15
EP0476078A1 (en) 1992-03-25
CA2047711C (en) 1996-01-09
ZA91943B (en) 1991-10-30
RU2046150C1 (en) 1995-10-20
CN1030720C (en) 1996-01-17
CA2047711A1 (en) 1991-08-24
GB2248632B (en) 1993-09-29
EP0476078A4 (en) 1993-02-24
MY105417A (en) 1994-09-30
EP0476078B1 (en) 1994-09-07
NZ237011A (en) 1992-06-25

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